CN110656485A - 一种天然抗菌防皱整理剂的制备方法 - Google Patents
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Abstract
本发明提供了一种天然抗菌防皱整理剂的制备方法,包括以下步骤:(1)在SiO2包裹的TiO2粉体表面修饰半琥珀酸酯;(2)将半琥珀酸酯的固体颗粒采用N‑羟基琥珀酰亚胺和碳二亚胺偶联壳聚糖;(3)向步骤(2)制得的溶液中加入聚乙二醇缩水甘油醚改性的丝素蛋白10‑20份、黄芩提取物10‑18份、甘草提取物12‑20份、鱼腥草15‑25份、交联剂5‑10份、表面活性剂4‑8份,在40‑60℃的温度下搅拌混合1‑2h,得到天然抗菌防皱整理剂。本发明所述整理剂对面料进行处理后使得面料具有良好的抗菌性和抗皱性,因此,采用本发明所述方法制得的整理剂在纺织领域具有重要的应用前景。
Description
技术领域
本发明属于纺织技术领域,具体涉及一种天然抗菌防皱整理剂的制备方法。
背景技术
随着人们生活水平的不断提高,人们的健康意识不断增强,具有抗菌、抗紫外、抗皱等多功能的新型面料的开发得到行业和研究工作者的普遍重视。这些多功能新型面料不仅能保证人体健康、防止外界环境对人体的伤害,还能够保证人体穿着的整洁度和美观性,从而提高面料的穿着性能。
纳米材料是近几年发展起来的一种新型材料,由于其具有独特的表面效应、小尺寸效应等特性,其在电子、涂料、医学、生物检测等领域具有广泛的应用前景,目前,纳米材料在纺织领域的应用研究也越来越普遍,然而现有的纳米材料对面料特性的改善并不理想,要想使得面料具有更好的功能性,需要进一步研究纳米材料以及与其他功能助剂的结合对面料所产生的影响,从而进一步提高面料的功能特性。
发明内容
为了解决以上现有技术存在的问题,本发明的目的在于提供一种天然抗菌防皱整理剂的制备方法。
为了实现上述目的,本发明提供以下技术方案:
一种天然抗菌防皱整理剂的制备方法,包括以下步骤:
(1)将SiO2包裹的TiO2粉体与琥珀酸酐以1:5-10的质量比加入无水吡啶溶液中,然后加入4-二甲氨基吡啶,4-二甲氨基吡啶与琥珀酸酐的摩尔比为1:10-15,将反应物在70-90℃的温度下搅拌反应3-6h后,将反应产物通过旋蒸去除有机溶剂,得到修饰有半琥珀酸酯的固体颗粒;
(2)将20-40份半琥珀酸酯的固体颗粒分散在pH6.0-6.5的缓冲液中使其质量分数为10-30%,在搅拌的条件下加入5-10份N-羟基琥珀酰亚胺反应10-20min,再加入10-15份碳二亚胺继续搅拌反应1-2h,最后加入40-60份20wt%的壳聚糖溶液继续搅拌反应4-8h,将反应产物使用pH6.0-6.5的缓冲液进行透析,得到修饰有壳聚糖的固体颗粒溶液;
(3)向步骤(2)制得的溶液中加入聚乙二醇缩水甘油醚改性的丝素蛋白10-20份、黄芩提取物10-18份、甘草提取物12-20份、鱼腥草15-25份、交联剂5-10份、表面活性剂4-8份,在40-60℃的温度下搅拌混合1-2h,得到天然抗菌防皱整理剂。
进一步的,所述pH6.0-6.5的缓冲液为2-(N-吗啉)乙磺酸缓冲液或磷酸盐缓冲液。
进一步的,所述步骤(3)中的交联剂为异氰酸酯或戊二醛。
进一步的,所述步骤(3)中的表面活性剂为脂肪醇聚氧乙烯醚(3)磺基琥珀酸单酯二钠、椰油酸单乙醇酰胺磺基琥珀酸单酯二钠或月桂醇醚磷酸酯的一种或几种组合。
进一步的,所述黄芩提取物、甘草提取物、鱼腥草均为水煎煮液,并通过活性炭吸附处理后制备而得。
进一步的,所述聚乙二醇缩水甘油醚改性的丝素蛋白的制备方法如下:
(1)将PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵溶于二氯甲烷中,50-60℃的温度下回流8-10h后过滤,将滤液使用二氯甲烷萃取2-3次,经无水硫酸钠干燥后减压蒸馏制得聚乙二醇缩水甘油醚;所述PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵的摩尔比为1:5:2:0.05;
(2)将聚乙二醇缩水甘油醚与质量分数为20%的丝素蛋白以1:2-5的质量比进行混合,在室温下搅拌混合1-2h,制得聚乙二醇缩水甘油醚改性的丝素蛋白溶液,并通过冷冻干燥制得聚乙二醇缩水甘油醚改性的丝素蛋白。
有益效果:本发明提供了一种天然抗菌防皱整理剂的制备方法,本发明所述整理剂以SiO2包裹的TiO2粉体为载体,并在其表面修饰壳聚糖,再辅以聚乙二醇缩水甘油醚改性的丝素蛋白以及其他功能性成分,从而制得具有良好抗菌性和防皱性的天然整理剂,本发明所述整理剂对面料进行处理后对金黄色葡萄球菌和大肠杆菌均有较好的抗菌性,同时急弹回复角高达334°,缓弹回复角高达365°,从而满足面料的抗菌性和抗皱性需求,因此,采用本发明所述方法制得的整理剂在纺织领域具有重要的应用前景。
具体实施方式
下面结合具体实施例来进一步描述本发明,但实施例仅是范例性的,并不对本发明的范围构成任何限制。本领域技术人员应该理解的是,在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换,但这些修改和替换均落入本发明的保护范围内。
以下实施例以及对比例使用的SiO2包裹的TiO2粉体参照“SiO2包裹改性对TiO2/环氧树脂涂膜防污抑菌性能的影响,DOI:10.3969/j.issn.1001-702X.2008.12.025”制备而得,其中所制备硅钛体系中,SiO2与TiO2的质量比为6%。
实施例1
一种天然抗菌防皱整理剂的制备方法,包括以下步骤:
(1)将SiO2包裹的TiO2粉体与琥珀酸酐以1:7的质量比加入无水吡啶溶液中,然后加入4-二甲氨基吡啶,4-二甲氨基吡啶与琥珀酸酐的摩尔比为1:12,将反应物在80℃的温度下搅拌反应4.5h后,将反应产物通过旋蒸去除有机溶剂,得到修饰有半琥珀酸酯的固体颗粒;
(2)将30份半琥珀酸酯的固体颗粒分散在pH6.0-6.5的缓冲液中使其质量分数为20%,在搅拌的条件下加入7份N-羟基琥珀酰亚胺反应15min,再加入13份碳二亚胺继续搅拌反应1.5h,最后加入50份20wt%的壳聚糖溶液继续搅拌反应6h,将反应产物使用pH6.0-6.5的缓冲液进行透析,得到修饰有壳聚糖的固体颗粒溶液;
(3)向步骤(2)制得的溶液中加入聚乙二醇缩水甘油醚改性的丝素蛋白15份、黄芩提取物14份、甘草提取物16份、鱼腥草20份、交联剂8份、表面活性剂6份,在50℃的温度下搅拌混合1.5h,得到天然抗菌防皱整理剂。
所述pH6.0-6.5的缓冲液为2-(N-吗啉)乙磺酸缓冲液。
所述步骤(3)中的交联剂为异氰酸酯。
所述步骤(3)中的表面活性剂为脂肪醇聚氧乙烯醚(3)磺基琥珀酸单酯二钠。
所述黄芩提取物、甘草提取物、鱼腥草均为水煎煮液,并通过活性炭吸附处理后制备而得。
所述聚乙二醇缩水甘油醚改性的丝素蛋白的制备方法如下:
(1)将PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵溶于二氯甲烷中,55℃的温度下回流9h后过滤,将滤液使用二氯甲烷萃取2-3次,经无水硫酸钠干燥后减压蒸馏制得聚乙二醇缩水甘油醚;所述PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵的摩尔比为1:5:2:0.05;
(2)将聚乙二醇缩水甘油醚与质量分数为20%的丝素蛋白以1:3.5的质量比进行混合,在室温下搅拌混合1.5h,制得聚乙二醇缩水甘油醚改性的丝素蛋白溶液,并通过冷冻干燥制得聚乙二醇缩水甘油醚改性的丝素蛋白。
实施例2
一种天然抗菌防皱整理剂的制备方法,包括以下步骤:
(1)将SiO2包裹的TiO2粉体与琥珀酸酐以1:5的质量比加入无水吡啶溶液中,然后加入4-二甲氨基吡啶,4-二甲氨基吡啶与琥珀酸酐的摩尔比为1:10,将反应物在70℃的温度下搅拌反应3h后,将反应产物通过旋蒸去除有机溶剂,得到修饰有半琥珀酸酯的固体颗粒;
(2)将20份半琥珀酸酯的固体颗粒分散在pH6.0-6.5的缓冲液中使其质量分数为10%,在搅拌的条件下加入5份N-羟基琥珀酰亚胺反应10min,再加入10份碳二亚胺继续搅拌反应1h,最后加入40份20wt%的壳聚糖溶液继续搅拌反应4h,将反应产物使用pH6.0-6.5的缓冲液进行透析,得到修饰有壳聚糖的固体颗粒溶液;
(3)向步骤(2)制得的溶液中加入聚乙二醇缩水甘油醚改性的丝素蛋白10份、黄芩提取物10份、甘草提取物12份、鱼腥草15份、交联剂5份、表面活性剂4份,在40℃的温度下搅拌混合1h,得到天然抗菌防皱整理剂。
所述pH6.0-6.5的缓冲液为磷酸盐缓冲液。
所述步骤(3)中的交联剂为戊二醛。
所述步骤(3)中的表面活性剂为椰油酸单乙醇酰胺磺基琥珀酸单酯二钠。
所述黄芩提取物、甘草提取物、鱼腥草均为水煎煮液,并通过活性炭吸附处理后制备而得。
所述聚乙二醇缩水甘油醚改性的丝素蛋白的制备方法如下:
(1)将PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵溶于二氯甲烷中,50℃的温度下回流8h后过滤,将滤液使用二氯甲烷萃取2-3次,经无水硫酸钠干燥后减压蒸馏制得聚乙二醇缩水甘油醚;所述PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵的摩尔比为1:5:2:0.05;
(2)将聚乙二醇缩水甘油醚与质量分数为20%的丝素蛋白以1:2的质量比进行混合,在室温下搅拌混合1h,制得聚乙二醇缩水甘油醚改性的丝素蛋白溶液,并通过冷冻干燥制得聚乙二醇缩水甘油醚改性的丝素蛋白。
实施例3
一种天然抗菌防皱整理剂的制备方法,包括以下步骤:
(1)将SiO2包裹的TiO2粉体与琥珀酸酐以1:6的质量比加入无水吡啶溶液中,然后加入4-二甲氨基吡啶,4-二甲氨基吡啶与琥珀酸酐的摩尔比为1:11,将反应物在75℃的温度下搅拌反应4h后,将反应产物通过旋蒸去除有机溶剂,得到修饰有半琥珀酸酯的固体颗粒;
(2)将25份半琥珀酸酯的固体颗粒分散在pH6.0-6.5的缓冲液中使其质量分数为15%,在搅拌的条件下加入6份N-羟基琥珀酰亚胺反应12min,再加入12份碳二亚胺继续搅拌反应1.2h,最后加入45份20wt%的壳聚糖溶液继续搅拌反应5h,将反应产物使用pH6.0-6.5的缓冲液进行透析,得到修饰有壳聚糖的固体颗粒溶液;
(3)向步骤(2)制得的溶液中加入聚乙二醇缩水甘油醚改性的丝素蛋白12份、黄芩提取物12份、甘草提取物15份、鱼腥草18份、交联剂6份、表面活性剂5份,在45℃的温度下搅拌混合1.2h,得到天然抗菌防皱整理剂。
所述pH6.0-6.5的缓冲液为2-(N-吗啉)乙磺酸缓冲液。
所述步骤(3)中的交联剂为戊二醛。
所述步骤(3)中的表面活性剂为月桂醇醚磷酸酯。
所述黄芩提取物、甘草提取物、鱼腥草均为水煎煮液,并通过活性炭吸附处理后制备而得。
所述聚乙二醇缩水甘油醚改性的丝素蛋白的制备方法如下:
(1)将PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵溶于二氯甲烷中,52℃的温度下回流8.5h后过滤,将滤液使用二氯甲烷萃取2-3次,经无水硫酸钠干燥后减压蒸馏制得聚乙二醇缩水甘油醚;所述PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵的摩尔比为1:5:2:0.05;
(2)将聚乙二醇缩水甘油醚与质量分数为20%的丝素蛋白以1:3的质量比进行混合,在室温下搅拌混合1.2h,制得聚乙二醇缩水甘油醚改性的丝素蛋白溶液,并通过冷冻干燥制得聚乙二醇缩水甘油醚改性的丝素蛋白。
实施例4
一种天然抗菌防皱整理剂的制备方法,包括以下步骤:
(1)将SiO2包裹的TiO2粉体与琥珀酸酐以1:10的质量比加入无水吡啶溶液中,然后加入4-二甲氨基吡啶,4-二甲氨基吡啶与琥珀酸酐的摩尔比为1:15,将反应物在90℃的温度下搅拌反应6h后,将反应产物通过旋蒸去除有机溶剂,得到修饰有半琥珀酸酯的固体颗粒;
(2)将40份半琥珀酸酯的固体颗粒分散在pH6.0-6.5的缓冲液中使其质量分数为30%,在搅拌的条件下加入10份N-羟基琥珀酰亚胺反应20min,再加入15份碳二亚胺继续搅拌反应2h,最后加入60份20wt%的壳聚糖溶液继续搅拌反应8h,将反应产物使用pH6.0-6.5的缓冲液进行透析,得到修饰有壳聚糖的固体颗粒溶液;
(3)向步骤(2)制得的溶液中加入聚乙二醇缩水甘油醚改性的丝素蛋白20份、黄芩提取物18份、甘草提取物20份、鱼腥草25份、交联剂10份、表面活性剂8份,在60℃的温度下搅拌混合2h,得到天然抗菌防皱整理剂。
所述pH6.0-6.5的缓冲液为磷酸盐缓冲液。
所述步骤(3)中的交联剂为异氰酸酯。
所述步骤(3)中的表面活性剂为质量比为1:1的脂肪醇聚氧乙烯醚(3)磺基琥珀酸单酯二钠。
所述黄芩提取物、甘草提取物、鱼腥草均为水煎煮液,并通过活性炭吸附处理后制备而得。
所述聚乙二醇缩水甘油醚改性的丝素蛋白的制备方法如下:
(1)将PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵溶于二氯甲烷中, 60℃的温度下回流10h后过滤,将滤液使用二氯甲烷萃取2-3次,经无水硫酸钠干燥后减压蒸馏制得聚乙二醇缩水甘油醚;所述PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵的摩尔比为1:5:2:0.05;
(2)将聚乙二醇缩水甘油醚与质量分数为20%的丝素蛋白以1:5的质量比进行混合,在室温下搅拌混合2h,制得聚乙二醇缩水甘油醚改性的丝素蛋白溶液,并通过冷冻干燥制得聚乙二醇缩水甘油醚改性的丝素蛋白。
对比例1
对比例1与实施例1的区别在于,对比例1中的TiO2粉体未经过SiO2包裹。
对比例2
对比例2与实施例1的区别在于,对比例2中未添加聚乙二醇缩水甘油醚改性的丝素蛋白。
将实施例1-4和对比例1-2制得的整理剂于室温下对纯棉面料采用二浸二轧的方式进行整理,轧液率为70%,然后于80℃预烘20min,再于120℃烘焙2min,制得整理后面料。
将整理后的面料进行性能测试,测试结果如表1所示,从表1中得出,经本发明所述整理剂整理的面料抗菌性和抗皱性能均良好,并且通过对比例得知,SiO2包裹的TiO2粉体对面料的抗菌性和抗皱性起到重要的作用,聚乙二醇缩水甘油醚改性的丝素蛋白对面料的抗菌性起到重要的作用。
表1
Claims (6)
1.一种天然抗菌防皱整理剂的制备方法,其特征在于,包括以下步骤:
(1)将SiO2包裹的TiO2粉体与琥珀酸酐以1:5-10的质量比加入无水吡啶溶液中,然后加入4-二甲氨基吡啶,4-二甲氨基吡啶与琥珀酸酐的摩尔比为1:10-15,将反应物在70-90℃的温度下搅拌反应3-6h后,将反应产物通过旋蒸去除有机溶剂,得到修饰有半琥珀酸酯的固体颗粒;
(2)将20-40份半琥珀酸酯的固体颗粒分散在pH6.0-6.5的缓冲液中使其质量分数为10-30%,在搅拌的条件下加入5-10份N-羟基琥珀酰亚胺反应10-20min,再加入10-15份碳二亚胺继续搅拌反应1-2h,最后加入40-60份20wt%的壳聚糖溶液继续搅拌反应4-8h,将反应产物使用pH6.0-6.5的缓冲液进行透析,得到修饰有壳聚糖的固体颗粒溶液;
(3)向步骤(2)制得的溶液中加入聚乙二醇缩水甘油醚改性的丝素蛋白10-20份、黄芩提取物10-18份、甘草提取物12-20份、鱼腥草15-25份、交联剂5-10份、表面活性剂4-8份,在40-60℃的温度下搅拌混合1-2h,得到天然抗菌防皱整理剂。
2.根据权利要求1所述的一种天然抗菌防皱整理剂的制备方法,其特征在于,所述pH6.0-6.5的缓冲液为2-(N-吗啉)乙磺酸缓冲液或磷酸盐缓冲液。
3.根据权利要求1所述的一种天然抗菌防皱整理剂的制备方法,其特征在于,所述步骤(3)中的交联剂为异氰酸酯或戊二醛。
4.根据权利要求1所述的一种天然抗菌防皱整理剂的制备方法,其特征在于,所述步骤(3)中的表面活性剂为脂肪醇聚氧乙烯醚(3)磺基琥珀酸单酯二钠、椰油酸单乙醇酰胺磺基琥珀酸单酯二钠或月桂醇醚磷酸酯的一种或几种组合。
5.根据权利要求1所述的一种天然抗菌防皱整理剂的制备方法,其特征在于,所述黄芩提取物、甘草提取物、鱼腥草均为水煎煮液,并通过活性炭吸附处理后制备而得。
6.根据权利要求1所述的一种天然抗菌防皱整理剂的制备方法,其特征在于,所述聚乙二醇缩水甘油醚改性的丝素蛋白的制备方法如下:
(1)将PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵溶于二氯甲烷中,50-60℃的温度下回流8-10h后过滤,将滤液使用二氯甲烷萃取2-3次,经无水硫酸钠干燥后减压蒸馏制得聚乙二醇缩水甘油醚;所述PEG、环氧氯丙烷、氢氧化钾、四丁基溴化铵的摩尔比为1:5:2:0.05;
(2)将聚乙二醇缩水甘油醚与质量分数为20%的丝素蛋白以1:2-5的质量比进行混合,在室温下搅拌混合1-2h,制得聚乙二醇缩水甘油醚改性的丝素蛋白溶液,并通过冷冻干燥制得聚乙二醇缩水甘油醚改性的丝素蛋白。
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